Oil treating process



April4, 1939. H. ROSENTHAL OIL TREAIING PROCESS 4 Sheets-She et.1

m vuwzwnzou led Aug. 4, 1934 /NVENTOR April 4, 1939- H. ROSEN'i'HAL' OIL TRE ATING PROCESS 4 Sheets-Sheet 2 Filed Aug. 4, 1934 INVENTOR April 4, 1939. H. ROSENTHAL OIL TREATING PROGE ISS 4 Sheets-Sheet 3 Filed Aug. 4, 1954 V MMDUE NVENTOR A ril 4, 1939. H. ROSENTHAL 2,152,664

OIL TREATING PROCESS Fild Aug. 4, 1934 4 Sheets-Sheet 4' INVENTOR Patented Apr. 4, 1939 1 UNITED STATES PATiiJ-LNT OFFICE 2,152,064 on. 'rnm'rmo rnoonss Henry Rosenthal, New York, N. Y. Application August 4, 1934, Serial No. 738,399

.8 Claims.

v ucts of high quality.

In the extraction of oil by solvent, the amount of solvent required to eflect substantially complete extraction depends upon the form of extractor and the method of extraction employed. During the extraction process an equilibrium exists between the oil in the solution and the oil in the solid material with which the solution is in immediate contact. To obtain eflicient operation, therefore, it is necessary -to move the solution in a counter-current direction to the movement' of the solid material in order that the fresh solvent contact the solid from which most of the oil has been removed. Furthermore, where the solution has specific gravity in excess of that of the solvent, the solution will tend to fall through the solvent so that the highest concentration of the solute will be at the bottom and the least concentration at the top of the solution. In order, therefore, to comply with the requirement of the spent solid contacting the least concentrated solution, it is desirable that the solvent generally move downward and that the solid generally move upward through the extract, and it is especially desirable that this general relation of movements take place as the solid is brought out of contact with the solution. It is further necessary that the movement of the solid inthe extractor be so regulated that the bed of solid in the extractor is not disturbed in such a way as to cause a compactionof material which will prevent a free flow of the solvent into the solid and of the solution out of the solid. I provide ap-' paratus for and methods of achieving these resuits as will be fully described in this specification.

As the solidmaterial leaves the extraction z one, it of course carries with it portions of the solution held by capillary attraction, absorption and entrainment. It is necessary to remove this solution from the spent solid for the purpose both of recovering the solvent and of recovering the spent material in suitable form. With such solvents as the low boiling hydrocarbons, I have discovered solvent from the spent meal prior to discharge of the meal from the extractor. In this way, any risk from fire is greatly reduced as solvent vapors are not discharged from the meal to the atmosphere.

6 Moreover, I have found that it is'desirable to separate from the discharged meal as much solvent as possible in the liquid form, as this requires the minimum expenditure of energy in recovering the solvent. after the maximum amount of solvent has been removed from the meal as liquid, further amounts be removed as vapor at such pressures that the vapors can be condensed by the application of the minimum amount of compression. It will then be necessary as a further step to reduce thepressure of the. vapor in contact with the meal after the solvent has been substantially vaporized in order to remove substantially all of the vapors.

Furthermore, it is desirable that 10 It is, also found desirable that the temperature 20 applied to the meal be limited in order to prevent deterioration of the meal.

My invention provides apparatus for and methods of accomplishing these results that will be more fully described.

The extraction of oil seeds and other materials requires that these materials be reduced to a meal in order that the solvent can penetrate to the oil cells. This meal contains finely pulverized particles. The solution on removal from the solid material often carries with it quantities of these particles, some of which may be in a substantially colloidal condition. This suspended materiahif left in the solution for any appreciable time, often ,causes the end product to deteriorate. Furthermore, many of the oils arevery viscous and diflicult to filter if the solvent is removed prior to the separation of the suspended material, which is often of a mucous or gelatinous character. I, therefore, provide a novel method comprising filtering the solution immediately upon its discharge from the extractor. To this end, I add to the solution prior to its discharge, such materials as diatomaceous earth "or other filter aid,

' where such is necessary, to assist in the removal of the suspended material which now may be easily filtered therefrom.

tial that all traces of solvent be removed from the that it isadvantageous to remove traces of the product. Even withsuch solventsaspropane and 8B butane, which are gases under normal temperature and atmospheric pressure, care is necessary in order that the final traces of solvent be eliminated, as the extraction of the oil from the solid depends upon the mutual solubility of the oil and the solvent, and this mutual solubility of the materials acts to prevent the ready removal of the solvent from the oil product. Furthermore, the application of high temperatures to efiect this separation in many cases causes a deterioration of the oil as the high temperature tends to produce undesirable color and to produce a dark colored oil. The proper handling of the solution will act to produce a product with desirablecolor characteristics. distillation tend to produce froth or foam when the oil content of the solution becomes sufliciently concentrated. This is especially true when small amounts of water are present. This irothing or foaming, unless properly provided for, prevents proper separation and acts to cause contamination of the condensed solvent. My invention provides a novel method of and means for efliciently separating the solvent and the product are thus i. To provide an emcient extraction.

2. To provide an extractor operable at other than atmospheric pressure.

3. To provide an efllcient means for removing solvent from the extracted meal.

4. To provide an extracted meal of high quality.

5. To provide an efiicient means for removing solvents from the solution.

6. To provide an oil of high quality.

'7. To provide methods of accomplishing the above objects continuously and uninterruptedly.

Other objects of my invention will be apparent from these specifications.

My invention will now be described in further detail by reference to the accompanying drawings which are part of these specifications. In these drawings:

Figure 1 is a diagrammatic layout bodiment of my invention.

Figure 2 is anelevation 01' one i'orm of my extractor.

of one em- Figure 3 is an and elevation of Figure 2, looking'from the left.

Figure 4 is an enlargement of portions of Figure 2 showing certain details. I Figure 5 is a section of Figure 4 on line AA. Figure 6 is a section of Figure 4 on line BB.

Figure '7 shows certain details of distilling apparatus shown in diagram in Figure 1.

Referring to Figure 1, the solid material to be extracted is fed into extractor I through rotary valve 2 from feed compartment 3 which is sealed to the atmosphere by the rotary valve 4 (see Fig-.

ure 2). The solvent is contained in the solvent storage tank 5 and is red to the extractor I through the solvent i'eed valve 6. The solution leaves the extractor through the discharge valve 1 and then passes by pipe 8 to the equalizing tank 9, equipped with level control It. The solution is withdrawn from the equalizing tank S'b'y the steam pump II, the supply of power of which is controlled by the level control Ill. Thus when the level of the solution rises in tank 9, steam valve I2 is opened \mder control of level control In and solvent is pumped out of the tank. when the level of solution in tank 9 lowers, the reverse takes place. The pump delivers the solution to the filter press 13, from. which the filtrate passes 75 by pipe line H to the heat exchanger IS. The

Furthermore, many oils upon from the solution. The objects of my invention which are not of a colloidal nature and which are not in solution in the menstruum being filtered.

In the heat exchanger IS, the solution is heated and is then delivered to the upper portion of the I still l'l. Still I! contains a plurality of steamheated trays with alternate distributing sections shown in greater detail in Figure '1. The solution enters the upper distributing section l8a and is discharged at the circumference over the serrated upturned vertical circumrerential edge Ma. The solution thus discharged from the distributing section l8a is delivered around the circumference of the steam-heated tray 20a. The

solution drains to the center of this tray and is discharged by the nipple Ma into the second distributing section l8b and continues in a like manner until it reaches the bottom of the still. In its passage over the heated trays, solvent is evaporated and the temperature of the solution increases as its concentration increases in its passage downward. The solution is heated only so long as it is in contact with the heated trays. Its time of contact with the heating means is therefore oi relatively short duration. Furthermore, the heating is done with the solution in thin flowing films. This has two advantages.

1. It prevents overheating, as the solution in thin films will tend to uniformly maintain the temperature corresponding with the pressure-in the still and the concentration of the solution at the instant.

2. The use of the thin films tends to limit any priming or foaming. Priming or foaming is not to be expected in the upper portion of the still, due to the relatively low concentration of the solution in the upper portions of the still. Any bubbles formed in the lower portion of the still will tend to be broken up before they reach the vapor outlet 22.

The concentrated solution from the lowest heating tray l8n is discharged to a pool 23 at the bottom of the still where it is out of contact with further heat. The level of this pool 23 is controlled by the level control valve 24, which maintains proper level in the pool by opening when a predetermined upper level is reached and closing when a predetermined lower level is reached. The amount of heating of the solution is controlled by the thermostatic'valve 25 which admits heating medium to the upper heating tray 20a. This thermostatic valve is controlled by the thermostat 26 in the pool 23. I

The material entering the still at the upper distributing section [811 is of course a solution of the extracted oil and this solution will have a relatively large amount of solvent of low boiling point. The vapor tension and vapor pressure of this solution at any temperature thus depend upon the mol percent of the solute and solvent in the solution. and the temperature of the solution. At any particular temperature, then, the vapor pressure and vapor tension will be at a maximum for the maximum moi percent 01' the low boiling component in the solution.

Conversely, if the pressure is substantially fixed, as it is in still I1 by its connection with condenser 30, the temperature of the solution is a minimum with the maxlmum'concentration of the low boiling component oi. the solution. Thus any attempt to addan increment of heat to the solution results primarily in vaporizing a arcades 3 heat so added appears largely as latent heat of vaporization and does not act to raise the temperature of the solution except as the vaporization acts to increase the concentration of the high boiling component of the solution.

As the concentration of the high boiling com-- ponent increases. progressivelyas the solution passes down the still and as the maximum concentration of the high boiling component is at the bottom of the still, the maximum temperature of the solution within the still will be at this location. Accordingly, I place the control of the heating medium at this location in order to accurately limit the maximum temperature of the solution.

Each heating tray, in order to easily withpipe 28a to the interior space 21b of the next lowest tray 20b and so continues down the still until it is discharged through pipe 29.

Vapor from the still I'I passes through pipe 22 to the condenser 30 where it is condensed and delivered to the solvent tank 3!. The pressure in still I1 is controlled by the pressure in condenser 30, which in turn depends upon the efficiency of the condenser, the temperature of the cooling water and the vapor pressure of the solvent. Where butane is used as a solvent, the pressure will in general be between 15 and 50 pounds per square inch gage, while with propane as the solvent the pressure will be in general between 50 pounds and 200 pounds per square inch gage. As the pressure of the still I! is controlled entirely by the condenser pressure, all vapors leaving the still leave at a pressure at which they are condensable without compression. The temperature of the solvent in condenser 30 may be above that of storage tank and extractor I. The pressure maintained in the condenser may, therefore, be in excess of themessure in the extractor. Pump H is provided to discharge the solution from the extractor through the filter l3 into. thestill l1 against such excess pressure as may exist.

The solution leaving the still I! through the level control valve 24 will have been freed from the principal amount of solvent and substantially all the solvent will have beenremoved from still I! that can be removed at the pressure of the condenser without exceeding limits of temperature which are controlled by the nature of the material being treated. This solution is discharged into the still 32. Still 32 is controlled at some predetermined pressure by means of the exhauster-compresson 33 which removes the vapors from still 32 as fast as they are generated and discharges them at condenser pressure either through valve 34 to condenser 30 where they are condensed along with the vapors from still IT, or through valve 35 to condenser 36 from which the condensed solvent is discharged to the solvent tank 3|. The suction pressure of the exhauster-compressor 33 is maintained at any predeterminedvalue by the control valve 31 which controls the supply of power to the compressor and is actuated by thepressure in the suction line to the compressor. I prefer that the pres:

sure in still 32 be maintained at substantially atmospheric pressure by this means.

In the extraction of certain oils some of the mucilaginous materials are partially soluble in the solvent. Such portions as'are soluble are therefore not removed by the filter l3 and will therefore be precipitated in the still l1. Where such soluble mucilaginous materials are present in suilicient amounts to be objectionable to the latter stages of the process they maybe removed by filtering means 38 after leaving the still l1 while the product still contains a certain amount of the solvent which aids in lowering the viscosity of the oil and thus acts to aid the rate of filtering.

The solution entering still 32 will be concentrated to such an extent that where the oil "solvent has been removed to materially increase the viscosity of the solution and that there still remains suflicient solvent so that its vapors will be present in such quantities as to form large and persistent bubbles. To prevent these bubbles from being carried with the vapor, I provide paddles 39 above the level of the solution in the still.

These paddles are operated by the motor 40 at sufficient speed to break the bubbles, as the paddles in rotation impinge against them. Also driven by the motor 40 is the mechanical stirrer ll immersed within the oil bath. This stirrer aids in the removal of the vapor from the so lution by mechanically dislodging the bubbles of vapor from the solution as they are formed and preventing the head of liquid in the bottom of the still from acting to keep such bubbles in the solution. 1

The still 32 is provided with the heating jacket 42. Heating medium, such as steam, is admitted within this jacket by means of thermostatic valve controlled by thermostat 44 within the still. The temperature of the oil in still 32 can thus be maintained at any predetermined value as described hereinbefore in connection with still Still 32 should be of such size that thesolution, in passing through it, is not maintained within the still and subject to the temperatures of the still any longer than is necessary for the removal of all but a very small percentage of solvent. A still of a size that, with normal flow of solution to and from the still, will hold the solution for less than fifteen minutes to one-half hour will generally be of proper size. The solution enters the still from the top and is discharged from the bottom through level control 46 to maintain a predetermined level of liquid in the still.

Certain oils, such as soy bean oil and lard, usually contain a very low content of free fatty acid and therefore, for many uses, refining with caustic is unnecessary with such materials. I have found that certain of these materials produce a light colored oil when extracted by my method without the use of a clarifying or bleaching agent. With other materials, it is sometimes desirable to bleach the material in order to secure a product of high quality. I provide means for doing this. Tank 41, equipped with agitator l3, driven by the motor 49, may thus contain a suspension of fuller's earth or activated carbon in some of the oil extracted in my process. Tank 41 is equalized in pressure with still- 32 through pipe 50, and its flow is controlled along with the a In fact, I have found that 'calLv through valve 64.

flow of liquid from the still 12 by means of level control 4 operating on the level control valve BI The liquid from tank 41 is thus mixed with the liquid discharge from still 32. As the liquid leaves still 32, it contains small amounts of solvent. This liquid is discharged by the pressure of still 32 into the vacuum still 52. This still is equipped with a motor driven stirrer and heatin jacket in the same manner as still 32, and where necessary may be provided with rotating paddles above the level of the liquid in the same manner as still 32. In addition, still 52 is equipped with a coil 53 having perforation N by means of which superheat steam may be admitted to the bath of oil at the bottom of the still. Still 52 is preferably maintained at a vacuum inches mercury by means of the condenser 55 and the exhauster-compressor 55. The temperature of the oil in the still 52 is controlled by thermostatic valve S'I which is actuated by the thermostat 58. Where open steam is used in coil 53, the temperature of the oil must be very closely controlled by means of thermostatic valve 51 as the temperature of the oil must be sufliciently high to prevent condensation of the steam in the -oil bath. While on the other hand, the temperature must be sufficiently low to prevent deterioration in the oil. The minimum temperature will, to an appreciable extent be governed by the vacuum maintained by condenser 55 and exhauster-compressor 56. With proper agitation of the bath, with temperatures of the 011 not exceeding 200 F. and a vacu *of26 inches of mercury, a complete removal of solvent may be obtained with only moderate use of open steam when either propane or butane is the solvent. the open steam is not necessary in some cases to ailect the solvent removal, but it should be available as a precautionary measure.

Condenser 55, operated at the pressure of still 52, is for the purpose of condensing the open steam added through coil 53. The vapors of solvent containing some moisture are withdrawn from this condenser by means of the exhauster II; which is operated to control the vacuum in the-condenser at any predetermined value. This control is effected by control valve 59 regulating the supply of power to the exhauster and actuated by the pressure in the suction line to the exhauster. The amount of solvent vaporshandled by exhauster it will be of insignificant amount when considered from the standpoint of their cost. They may. therefore, be discharged from the system through valve SI at substantially atmospheric pressure or they may be discharged through valve 6| to condenser 62 from which they are delivered through solvent tank 3| to separator 63, which separator is provided to separate the water condensed along with the vapor in condenser 62. This water is drawn oi! periodi- The oil is removed from the pump 65, the operation of which is .controlled by valve 68, actuated by the level controlt'l. In this manner a predetermined level of liquid-is maintained in still 52. The oil pumped from still 52 is discharged through heat exchanger l5, oil cooler 69 to the oil storage tank 10. Where the oil discharged from still 52 is not clear and brilliant, it may be passed through filter 88 before being cooled in the heat exchanger i5 and the cooler 69.

The solvent from tank is returned to the storage tank. 5 by means of the pump II. This of from 24 to 28 tem. This 011 still 52 by means or pump maintains a predetermined level or liquid in tank ll by means ofthe control valve 12 and the level control 13.

.- The solvent in tank I is preferably held within a predetermined range of temperature, this range depending upon' the material being extracted and the quality of product desired. Thermostat ll within the storage tank controls thermostatic valves "and-18. Valve 15 controls the compressor I! and allows the compressor to operate and withdraw'solvent vapors from thestorage tank when the temperature of the solvent reaches the predetermined upper level. The solvent is thus cooled by evaporation and the vapors drawn oil are compressed, condensed in condenser Il, and returned to the storage tank 5. If the extraction is being conducted at a temperature in excess of atmospheric temperature, thermostatic valve 16 is opened when the solvent reaches a predetermined minimum value and heating medium is admitted to coil 19.

Now referring more specifically to Figures 2, 3, 4, 5 and 6, the details of the extractor proper will be explained. 4

The solid materials entering through the rotary valve 4 are discharged to the feed compartment 3, which is maintained at substantially atmospheric pressure by means of the outlet pipe which connects with the vapor recovery system 8| (see Figure l) Feed compartment 3 will contain a certain amount of vapor which is admitted from the extractor through rotary valve 2 and a certain amount of air which is admitted into oil to the vapor recovery system. Thus, a large .4:

portion of the vapors admitted to the inlet compartment 3 will be condensed and absorbed by the charge of solids and will be fed back directly to the extractor and will thus not have to be recovered in the vaporrecovery system. i

The vapor recovery system 8! may be any well known type and may utilize either the principle I of liquid absorptiomor the principle of solid absorption. -However,' I prefer that liqui tion be used and that the absorption medium be devolati lized oil produced in the extraction sysaifter being used to absorb the solvent vapors may be returned to the main extractor system either through still I! or still 32.

The extractor, a stationary horizontal cylindrical shell 82 with dished heads 83 and 84, is divided into a number of compartments 85a, 85b, etc., in which the mealis contacted with the solvent; Each compartment is formed by the cylindrical shell of the extractor and a pair of diaphragms in the lower half of the extractor. These diaphragms are illustrated at 86a, 861), etc. The diaphragms 86aand 86b, together with the shell, form compartment 850..

As shown in Figure 6, each its upper portion a bearing 81a, 81b, etc., supporting the shaft 88 which extends through the extractor head 83-. The opening, through which the shaft extends, is sealed by means of the stuffing box 89, mounted on head 83. Within each compartment 85 and supported from shaft 88 by means of the spiders 90 there is a rotating cylinder 9| (Figure 5). This cylinder is composed of perforated metal of suitable size to support the solid material being extracted. This cylinder diaphragm has on d absorptroughs formed by the corrugations.

Swipe 96 (Figure 6).

has a smooth exterior so that on rotation it can fit snugly against a semi-circular diaphragm lying in the lower half of compartment 85. This diaphragm 92 shown in cross section in Figure 5 is composed of three segments. The two outer segments 92a constructed of a solid sheet of metal will prevent free flow of liquid from the cylinder 9| into the annular space between the cylinders 9| and 82. The lower portion, 92b of the diaphragm, however, is a corrugated sheet on which cylinder 9| rests only on the upper edges, thus allowing the liquid to pass freely through the perforations of cylinder 9| down into the Here the solution is drained down the holes 93, from which it passes into the annular space between cylinders 9| and 82. I

On the spider 90, adjacent to the point at which the spider is sealed against the vertical diaphragms 86, are series of buckets 94. These buckets rotate with the cylinder 9| and are located in the annular space between this cylinder and the extractor cylinder 82. Each bucket is equipped with a discharge pipe 95 and an inlet Also mounted on the spider, but on the inside of cylinder 9|, are the vanes 91 which rotate with the spider and effect the movement of the solid material. On each of the vertical diaphragms is the deflector vane 98a, 98b, etc. These vanes are mounted on shafts 99a, 99b, etc. mounted in trunnions supported by the main bearing 81. Shaft 99 is placed between the rotating cylinders and extends through the extractor shell 82 by means of the stufling box IOI. Th shaft is equipped with a. handle I02 by means of which it can be rotated and the positions of the vane 98 may be adjusted thereby. Also between the cylinders 9| and mounted above the vane 98 is the trough I03 supporting the pipe I04 with the spray head I05. Trough I03 is provided with a shaft at either end, one shaft I04 being mounted pn the bearing I05 fixed from the cylinder 82.. The shaft I06 at the other end, passing through stufling box I01, is equipped with handle I08. By means of this handle the position of the trough can be adjusted. In addition to the compartments 85a, 85b, etc., in which are mounted the rotating cylinders 9Ia, 9Ib etc., there is a compartment at either end of the extractor. Compartment I09 (Figure 4) serves to retain the solution which is about to be discharged from the extractor. enters compartment I09 through the series of holes in diaphragm 860.. In this compartment I09, mounted on the shaft 88, are the paddles III. Pressure tank II2 with rotary valve II3 delivers into (see Figure 2) compartment I09 by means of pipe I I4. This tank may be used to hold a suspension of filter aid which on delivery to compartment I09 is incorporated by means of the paddles I II with the solution in the compartment.

At the other end of the extractor is compartment H with the paddles H6 mounted on the shaft 88. Compartment II5 has a bottom opening entering upon the conveyor chamber I I 1 containing the screw conveyor I I8. The paddles 6 are provided to deliver the extracted solid ma-' terials into this opening.

Conveyor chamber II 1 is provided with a hea ing jacket II9. Heating medium is admitted through this chamber by means of the thermostatic valve I20 (see Figure 1) operated by the thermostat I2I in the conveyor compartment at a point where the spent meal is discharged from This solution a the conveyor into the rotary valve I22. Rotary valve I22 serves to discharge the meal into the discharge compartment I23 which is maintained under high vacuum by suction applied through the pipe I24, which preferably leaves through valve I25 to the vapor recovery system 8| (Figure 1). Meal is discharged from the discharge compartment I28 by means of the'rotary valve partment 85a. Vanes 91 mounted on rotating a cylinder 9Ia carry these solids forward through the solvent in the compartment and they are finally discharged onto the deflector 9811 from which they are delivered to the second compartment of the extractor. This operation is repeated in the second compartment and is continued through as many stages as are necessary to complete the extraction. As shown in Figure 2, there are four extracting compartments 85a, 85b, 85c and 85d. The solids from 85d are carried into compartment 85c to which no solvent is fed so that in this compartment thesolid material is freed from liquid by draining. The drained solids are then carried forward to compartment II5 where the paddles II6 act to push the solids into the conveyor chamber III. The conveyor carries the" solids through the heated conveyor chamber to the rotary discharge valve I22. As the conveyor chamber and the ex-, tractor compartments are in open communication and at the same pressure, little increase in temperature of the meal in the conveyor chamber is necessaryto efiect complete vaporization of the solvent. The addition of the heat necessary to supply the heat of vaporization can therefore be closely controlled by the thermostat I2I.

It will be noted that the vanes 91 which move the meal within a single extractor compartment, act to lift the solid material from the bottom of the bath and carry it upward through the solvent in the compartment, to which solvent is delivered to the top of the bath and is discharged from the bottom of "the bath. This general upward movement of the meal is most pronounced atthe point where the solid is being discharged from the one compartment to the next. There is thus a down-flow of solvent and an up-flow of solid as the solids are being discharged.

Fresh solution is fed into the extractor into the second section before the solid is discharged. Thus, as shown in- Figure 2, it is fed in the compartment 85d. through the bed of solid, extracts the oil therefrom and passes out of the rotating cylinder containing the solid material into the annular space which surrounds the rotating cylinder. The buckets provided around the outside circumference of the rotating cylinder pick up the solution in the bottom of the annular space and lift it so that it may be discharged'into the trough I03 and so into the next compartment in a direction counter-flow to that,of the solid material.

The solution in passing The flow of liquid from one compart ment to another .may be adjusted by changing the position of the trough I03 with its connecting pipe and nozzle. If the trough is tilted toward the compartment from which the liquid is being lifted, a portionoi' the liquid will flow back into that compartment. If tilted in the opposite direction, allof the solution will be delivered to the next forward compartment. In this way the flow of liquid and the height of the solutionvin each compartment can be adjusted. I prefer to operate with asolution level in each compartment, somewhat below the bottom of the'shaft by which the cylinders are supported and turned.

In a like manner the deflector vanes '98 may be tilted and the movement of the solid material through the extractor can be controlled and the level of solid in each of the compartments adiusted. I prefer that the level of solids be maintained just below the center line of the extractor.

As has previously been mentioned, the last rotating cylindrical compartment before the discharge of the meal is operatedwith no solution flowing thereto. The movement of meal through this compartment over the perforated metal shell of the rotating cylinderpermits the meal to be .drained of all extraneous solvent before it is delivered to the heated screw conveyor by means of the paddle in the end compartment of the extractor cylinder from which the solids are delivered. The rotating cylindrical compartment in which the solvent is drained from the solids is equipped with a series of buckets for lifting the solvent from below the cylinder in the same manner as the other rotating cylinders. These buckets keep the level oithe solvent in this compartment belowthe level of the bottom of the rotating screen and deliver the solvent drained through the screen into the adjacentrotating cylinder along with the fresh solvent being delivered to the extractor.

The spent meal, as it enters the screw coniveyo is thus relatively dry. In this conveyor sufiicient heat is added to completely vaporize the solvent which remains in the meal. A substantial portion of the vapors thus generated condense in the solution within the extractor cylinder, but a portion of the solvent vapors remain with the meal at extractor pressure. The amount of heat added while the meal passes through the conveyor must be suflicient to supply the latent heat of vaporization of the entrained liquid solvent, to slightly raise the temperature of the meal and to somewhat superheat the solvent vapor. Where propane and butane or similar low boiling hydrocarbons are used as solvents, the temperature at which, the

I heat is added and to which the meal and vapors must be heated is low and need not exceed F. The heating stage for solvent removal from the mealis therefore low. Furthermore, the meal is heated 'out of contact with air or oxygen. 'Thus, in the handling of either vegetable or animal material, the proteins contained therein are 5 neither-converted by heat nor oxidized by air ,ing conveyor into the rotaryvalve, is accompanied by an amount of solvent vapors in the interstices of the meal. moved by reduction in pressure. This is e pecially true when low boiling hydrocarbons; which have the property of superheating on expansion,

7'5 are used as solvents. There is thus no tendency This vapor may be refor recondensation when the meal with its entrained vapor passes from the conveyor at extractor pressure through the rotary valve to the discharge chamber wherelow pressure. is maintained.- The pressure maintained in the discharge chamber should be less than half of atmosphere, and I prefer that it be from 24 to 28 inches of mercury. This reduced pressure may be maintained by any well known means. I prefer that the solvents removed from the discharge chamber be delivered to a solvent recovery system, preferably of the oil absorption type. and that the recovered solvent be returned to the extractor system.

In the preceding, I have described the details of an .oil extraction and separation wstem. It will be obvious that numerous products may be treated in my system for extracting oils, and that numerous oils in solution may be separated in accordance with my invention, the physical conditions being varied in accordance with the product being treated.

In my copending applications filed of even data relating to Methods and prcdu'ctsof cotton seed extraction; Serial Number 738,402;

ment thereof, Serial Number 738,404, now Patent Number 2,123,207, I have disclosed certain specific applications of my invention although it will be understood thatit'may equally well be applied to the numerous other edible extracted oils.

In my copending application filed of even date relating to Extraction of oil shale, Serial Humber 738,405, I have disclosed application of the extractor described and claimed in this application to a specific petroleum oil, but it will be understood that the invention is equally applicable to the extraction and separation of ,petroleum soaked sands and similar materials.

Thus it will be understood that the invention may be applied to extraction of many products, and that the refining of oils generally may be carried on in accordance with'theprinciples 01 my invention, and I do not intend to limit myself except as set forth in the appended claims I claim:

' 1. In a system of continuous extraction, a closed extractor having a plurality of substantially horizontal perforated cylindrical compartments, an adjustable deflector positioned betweer adjacent compartments, each compartment being provided with a seriesof blades attached to the inner circumference of said cylinder, said blade: being adapted to raise solid material lying within said cylindrical compartment to propel saic solid material longitudinally of said, compartment, and finally to raise said solid material an: discharge same to said adjustable deflector iron which said solid material is discharged to an adjacent cylindrical compartment, and means or the exterior of said closed extractor for controlling said adjustable deflector within said extractor.

' 2. In a system of cutinuous extraction, a sub stantially horizontal extractor having a pluralit: of perforated cylindrical rotatable compartments each compartment being provided at one em with a series of buckets attached to the outer circumference of said cylinder and rotatable witl same, said buckets being adapted to raise solution from a space within the extractor belov said cylinder and deliver said liquid to a trougl placed transversely of said extractor and mount ed externally of said cylindrical compartment,' 6. A continuous extractor comprising a horiand means for delivering said solution from said trough to the adjacent cylindrical compartment.

3. In a system 01' continuous extraction, a substantially horizontal extractor provided with a plurality of diaphragms forming compartments within said extractor, a plurality of perforated cylinders rotatable within said compartment, means for moving a bed of solid material contained within said rotating cylinders, means secured to the exterior of said cylinders and operable with said cylinders for moving solution contained within said compartments, adjustable deilectors mounted above said diaphragms and means for elevating said solid material above said deflectors, whereby the how of solid material from one compartment to an adjacent compost meat may be controlled, and troughs mounted above said diaphragms whereby the flow of solution from one compartment to an adjacent compartment may be controlled. I

d. In a system of continuous extraction, a substantially horizontal extractor provided with a plurality of cylindrical rotatable compartments, means for delivering solution from one of said cements to an adjacent compartment, a separate stationary end compartment into which the solution about to be discharged from said extractor is delivered, means for delivering solution from a rotatable compartment to said end compartment, means in communication with said end.

compartment for delivering a filter-aid to the solution contained in said compartment, and means within said compartment rotatable with said rotatable compartments for mixing said filter-aid into said solution.

5. In a'system of continuous extraction, means for charging solid material to an extractor operating at superatmospheric pressure, said means comprising a chamber sealed at either end by means of a substantially tight displacement valve adapted to form a closure while delivering solids and provided with a vapor outlet near the upper portion of said chamber for the eduction oi solvent vapors from the sealed space, means in communication with said vapor outlet for removing and compressing vapors, whereby solvent vapors carried from the extractor into said chamber are passed through the solid material in said chamher before being discharged and a portion of said vapors are absorbed in said solid material and returned to said extractor, and whereby the pressure in said chamber is maintained at some predetermined value.

zontal stationary cylindrical shell. capable of withstanding superatmospheric pressure. a plurality of vertical diaphragms dividing said shell into a plurality of interior compartments, semicircular horizontal diaphragms in the lower portion of center interior compartments, said horizontal diaphragms being smooth on their upper portions and corrugated on their lower portions, a horizontal rotatable shaft supported by said vertical diaphragms and carrying a plurality of horizontal perforated cylindrical shells so mounted that their circumferences are substantially in contact with said horizontal diaphragms, means for admitting solids to the interior of the extractor, means for advancing said solids through the extractor, means for discharging said solids from the extractor, and means for admitting solvent to the extractor and removing solution from the ear-- tractor.

7. In a continuous-extraction system, an. extractor comprising a sealed inlet chamber, an elutriation zone having a plurality of rotating chambers, a chamber for. vaporizing solvent asso ciated with the spent meal, said latter chamber consisting of a screw rotating in a heated cylinder connected with the elutriation zone in a manner that the vapors released from the meal having a lesser amount of solvent pass through the meal having a. greater amount of solvent and are discharged from the vaporizing chamber into the 'elutriation zone, a sealed outlet chamber, and connections for admission of solvent to the extractor and for discharge of solution from the extractor.

8. The method of continuous extraction of oleaginous substances which comprises contacting oleaginous and protein containing solid material with a liquid hydrocarbon solvent, that is gaseous at normal temperature and pressure, under superatmospheric pressure at which said solvent is maintained in liquid state, to dissolve the oleaginous substances; withdrawing the solution so formed from the remaining solid material; and substantially completely evaporating the solvent under superatmospheric pressure and at a temperature of the order 0! F. from the protein containing solid remaining after extraction, while maintaining the substantially oil-tree protein residue in an atmosphere of solvent vapor substantially free from moisture.

HENRY ROSEN'I'HAL. 

